CN109516679A - A kind of middle infrared lumious material of rare earth ion doped devitrified glass and preparation method thereof - Google Patents
A kind of middle infrared lumious material of rare earth ion doped devitrified glass and preparation method thereof Download PDFInfo
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- CN109516679A CN109516679A CN201910011726.8A CN201910011726A CN109516679A CN 109516679 A CN109516679 A CN 109516679A CN 201910011726 A CN201910011726 A CN 201910011726A CN 109516679 A CN109516679 A CN 109516679A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
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Abstract
The present invention discloses a kind of middle infrared lumious material and preparation method thereof of rare earth ion doped devitrified glass, and the material is by including rare earth ion Er3+And Bi3.20Te0.80O6.40The tellurium bismuthates devitrified glass of nano-crystalline granule is constituted, and first prepares Er containing rare earth ion3+Tellurium bismuthate glass, then glass is made up containing Bi of two-step thermal processing technology3.20Te0.80O6.40Nanocrystalline devitrified glass.Resulting devitrified glass has good optical property, is irradiated by exciting light, utilizes the rare earth ion Er in the low phonon energy environment of nanocrystalline construction3+Realize efficient 2.7 μm of fluorescence radiation.
Description
Technical field
The present invention provides the middle infrared lumious material and preparation method of a kind of rear-earth-doped devitrified glass, belong in it is infrared
Luminescent material technical field.
Background technique
2-5 mu m waveband fluorescence has relatively high transmitance in an atmosphere, can be utilized for optic communication transmission, is applied to
Communication, national defence, the fields such as satellite remote sensing.In addition to this, 2-5 mu m waveband fluorescence is very polymolecular characteristic absorption frequency range, this allows
Middle IR fluorescence has wide application in air monitoring, industrial procedure control, the environment protection fields such as pollutant leakage monitoring
Prospect, while middle IR fluorescence can also be applied to drug surveillance, medical diagnosis, the medical fields such as laser surgey.
Tellurate glass has wide infrared transmission window, low melting point, good stability and durability, in a low voice sub- energy
Amount, high refractive index, good non-linear optical property, excellent infrared breathability and rare earth ion doped content height etc. are excellent
Point, it is considered to be IR fluorescence luminous host in ideal.Er3+Possess level structure abundant in crystalline field, it not only can be with
By ultraviolet light and excited by visible light, can also be excited by the commercial pump light that wavelength is 808nm and 980nm.In pump light source
Under excitation, Er3+Ground state level electronics can transit to excitation state by ground state absorption mode, and the electronics in excitation state passes through4I11/2→4I13/2The middle IR fluorescence output that energy level transition generation wavelength is about 2.7 μm.
In order to realize high efficiency, the output of high-power laser, people have begun to all kinds of solids from the 1960s
The development of laser, host material relate generally to laser crystal and glass.But both host materials have the defect of itself, brilliant
Body material preparation condition is more harsh, and is not used to drawing optical fiber, limits its further application；Common quartz glass hair
Light efficiency is lower, higher phonon energy (1100cm-1) limit the energy conversion efficiency of laser, the Intrinsic Gettering of matrix
The laser output of middle infrared band is limited, the requirement for preparing laser is unable to satisfy.In order to obtain excellent luminescent properties with
And good environmental suitability, the material for rare earth ion doped luminous host do not require nothing more than it with lower phonon energy
Amount, and require it with good thermal stability, chemical stability and mechanical performance.Devitrified glass, being will be special by control
Surely polycrystalline solids material of the one kind prepared by the parent glass crystallization formed containing a large amount of crystallite phases and glass phase, is provided simultaneously with
Some performances of crystal and glass, can be in combination with Er3+Doped crystal material luminous efficiency height and easy to process excellent of glass
Point.Compared with monocrystal material, the preparation process of devitrified glass is relatively easy, and short preparation period is at low cost；With composite material phase
Than the index matching of crystal and mother glass is good in devitrified glass, realizes that device is assembled without integration packaging, will not generate
Bubble greatly reduces cost and the time of production technology.
Summary of the invention
The object of the present invention is to provide infrared lumious material and preparation method in a kind of rear-earth-doped devitrified glass, the rare earths
The middle infrared lumious material of doped microcrystalline glass is by including rare earth ion Er3+And Bi3.20Te0.80O6.40The tellurium bismuth of nano-crystalline granule
Hydrochlorate devitrified glass is constituted, and first prepares Er containing rare earth ion3+Tellurium bismuthate glass, then by two-step thermal processing technology by glass
Glass is made containing Bi3.20Te0.80O6.40Nanocrystalline devitrified glass.
A kind of middle infrared lumious material of rear-earth-doped devitrified glass, the component of the middle infrared lumious material is as follows, base
This raw material composition: TeO265~90mol%、Bi2O35 ~ 15 mol % and Nb2O55 ~ 20 mol%, said components and be 100mol%,
In addition it adulterates: Er2O3, doping is the 0.2-0.75mol% of aforementioned basic raw material composition.
Another object of the present invention is to provide the preparation methods of infrared lumious material in rear-earth-doped devitrified glass, first make
Standby Er containing rare earth ion3+Tellurium bismuthate glass, then glass is made up containing Bi of two-step thermal processing technology3.20Te0.80O6.40
Nanocrystalline devitrified glass.Specifically comprise the following steps:
(1) raw material is sufficiently mixed, stirring carries out melted, and the liquid of melting is poured into stainless steel punching block, Muffle is then placed in
It anneals after furnace heat preservation, then cools to room temperature, obtain the glass containing rare earth ion, and obtained glass is cut
And polishing treatment；
(2) glass containing rare earth ion after polishing treatment is heat-treated in Tg ± 2 DEG C, then proceedes to heating lower than crystallization temperature
2-5 DEG C of heat treatment of degree, cooled to room temperature is to get the infrared lumious material into the rear-earth-doped devitrified glass.
Further, in the step (1), glass melting temperature is 800 ~ 1000 DEG C, and melting time is 30 ~ 60min.
Further, in the step (1), stainless steel punching block is preheated to 200 ~ 350 DEG C.
Further, in the step (1), temperature is 370 ~ 390 DEG C in Muffle furnace, keeps the temperature two hours.
Further, in the step (1), cooling velocity is 5 ~ 10 DEG C/min.
Further, in the step (2), 8-12h is heat-treated in glass transition temperature.
Further, in the step (2), it is being lower than 2-5 DEG C of heat treatment 90-180min of crystallization temperature.
In order to optimize Er3+The design of doped microcrystalline glass material, in tellurate (750cm-1) joined than its sound in glass
The sub- lower Bi of energy2O3To reduce the phonon energy of matrix, it is easier to realize the radiation transistion of electronics, Nb is added2O5Improve it
Refractive index matches glass matrix more with the refractive index of nano-crystalline granule, scattering is reduced, to further increase Er3+It shines
Efficiency.
Based on this, we have selected TeO2-Nb2O5-Bi2O3-Er2O3Glass system prepares Er as presoma glass3+
Doping includes Bi3.20Te0.80O6.40Nanocrystalline tellurate microcrystalline glass,.Have studied Er3+In in transparent tellurium bismuthate glass
The characteristics of luminescence of infrared aspect, the material are expected to the gain medium material as mid-infrared fiber laser, can be efficient for preparation
Rear-earth-doped glass in infraluminescence new thinking and approach are provided.
The invention has the benefit that
(1) infrared lumious material in rear-earth-doped devitrified glass of the present invention has both the low phonon energy environment and glass of crystal
Low scattering, low-loss, chemistry and the mechanically stable characteristic of glass；
(2) the method for the invention can effectively control the particle size of tellurium bismuth oxide crystallite, and guarantee the tellurium bismuth oxide
The size of crystallite is in nanoscale range (5-15nm), so that made devitrified glass keeps good translucency；
(3) the method for the invention uses two-step thermal processing, and infrared lumious material has in rear-earth-doped devitrified glass obtained
Good optical property, is irradiated by exciting light, using the local field enhancement effect of tellurium bismuth oxide nanocrystalline, is made in a low voice
Rare earth ion in sub- energy realizes that efficient middle IR fluorescence shines, and luminous efficiency has obvious increasing compared to host glass
By force；
(4) of the invention containing infrared rare earth luminescent material in nanocrystalline devitrified glass, efficiently conversion is obtained for preparing
Infrared lumious material has certain directive significance in the commercialization of pump energy.
Detailed description of the invention
Fig. 1 is differential thermal (DTA) test curve of the tellurium bismuthate glass containing rare earth ion in embodiment 1；
Fig. 2 is the XRD spectrum for the er-doped tellurium bismuthates devitrified glass that embodiment 1 obtains；
Fig. 3 a is the transmission electron microscope TEM figure for the er-doped tellurium bismuthates devitrified glass that embodiment 1 obtains；
Fig. 3 b be the obtained er-doped tellurium bismuthates devitrified glass of embodiment 1 and electron diffraction diagram；
Fig. 4 is infraluminescence map in 2.7 μm of the er-doped tellurium bismuthates devitrified glass that embodiment 1 obtains；
Fig. 5 is the XRD spectrum for the er-doped tellurium bismuthates devitrified glass that embodiment 2 obtains；
Fig. 6 is infraluminescence map in 2.7 μm of the er-doped tellurium bismuthates devitrified glass that embodiment 2 obtains；
Fig. 7 is infraluminescence map in 2.7 μm of the er-doped tellurium bismuthates devitrified glass that embodiment 3 obtains；
Fig. 8 is infraluminescence map in 2.7 μm of the er-doped tellurium bismuthates devitrified glass that embodiment 4 obtains.
Specific embodiment
Invention is described in further detail with reference to embodiments, but the scope of the present invention is not limited to the content.
Embodiment 1
By composition 75TeO2-12.5Nb2O5-12.5Bi2O3(mol%) TeO needed for weighing 60g2, Nb2O5, Bi2O3, Er2O3Powder
Raw material (purity 99.99%), Er2O3According to 0.75mol% is mixed outside molar ratio, it is fitted into crucible with cover and is placed in after being sufficiently mixed
Glass solution, is then quickly cast on the Stainless Molding Board for having been preheated with 200 DEG C by 850 DEG C of melted 30min, after molding
Two hours are kept the temperature for 380 DEG C in Muffle furnace, and temperature is cooled to by room temperature with the speed of 5 DEG C/min, obtains the tellurium bismuth containing rare earth ion
Silicate glass, and obtained glass cut, polishing treatment；By the obtained tellurium bismuthate glass containing rare earth ion
400 DEG C of heat treatment 10h(glass transition temperature Tg=398 DEG C), then 425 DEG C of heat treatment 180min(crystallization temperature Tc=428
DEG C), cooled to room temperature to get arrive transparent glass-ceramics.Under similarity condition, replace with 120 in 425 DEG C of heat treatment times,
100 and 0min.
From fig. 1, it can be seen that the glass transition temperature of the tellurium bismuthate glass containing rare earth ion is 398 DEG C, crystallization temperature
It is 428 DEG C.Infrared lumious material has good translucency in rear-earth-doped devitrified glass described in the present embodiment, as can be seen from Figure 2
The devitrified glass has apparent crystallization to show, and compareing crystallization substance according to xrd card is Bi3.20Te0.80O6.40.It was found from Fig. 3 a
Nanocrystalline size is 5-15nm in the material, and nanocrystal is evenly distributed in substrate glass, be can see from Fig. 3 b
There is diffraction spot in diffraction pattern, further demonstrates the precipitation of crystal.From rare earth ion known to the luminous map of Fig. 4 in crystallite
Luminous intensity has been up to 2.5 times of the glass material without Overheating Treatment in glass environment.
Embodiment 2
By composition 75TeO2-12.5Nb2O5-12.5Bi2O3(mol%) TeO needed for weighing 60g2,Nb2O5,Bi2O3,Er2O3Powder
Raw material (purity 99.99%), Er2O3According to 0.5mol% is mixed outside molar ratio, it is fitted into crucible with cover and is placed in after being sufficiently mixed
Glass solution, is then quickly cast on the Stainless Molding Board for having been preheated with 200 DEG C by 850 DEG C of melted 30min, after molding
Two hours are kept the temperature for 380 DEG C in Muffle furnace, and temperature is cooled to by room temperature with the speed of 5 DEG C/min, obtains the tellurium bismuth containing rare earth ion
Silicate glass, and obtained glass cut, polishing treatment；By the obtained tellurium bismuthate glass containing rare earth ion
In 400 DEG C of heat treatment 10h, then in 425 DEG C of heat treatment 180min, cooled to room temperature is to get arriving transparent glass-ceramics.Together
Under the conditions of sample, 120,100 and 0min is replaced in 425 DEG C of heat treatment times.
Infrared lumious material has good translucency in rear-earth-doped devitrified glass described in the present embodiment, as can be seen from Figure 5
Crystal has been precipitated in the material, through Scherrer formula calculate the size of crystal is also Nano grade, and nanocrystal is in matrix glass
It is evenly distributed in glass (referring to Fig. 3), from rare earth ion luminous intensity in the environment of nanocrystal field known to the luminous map of Fig. 6
It has been up to 2 times of the glass material without Overheating Treatment.
Embodiment 3
By composition 65TeO2-20Nb2O5-15Bi2O3(mol%) TeO needed for weighing 60g2,Nb2O5,Bi2O3,Er2O3Powder raw material
(purity 99.99%), Er2O3According to 0.4mol% is mixed outside molar ratio, it is fitted into after being sufficiently mixed in crucible with cover and is placed in 1000 DEG C
45min is melted, is then quickly cast to glass solution on the Stainless Molding Board for having been preheated with 200 DEG C, in Muffle after molding
Two hours are kept the temperature for 380 DEG C in furnace, and temperature is cooled to by room temperature with the speed of 10 DEG C/min, obtains the tellurium bismuthates containing rare earth ion
Glass, and obtained glass cut, polishing treatment；The obtained tellurium bismuthate glass containing rare earth ion is existed
400 DEG C are nearby heat-treated 10h, and then in 423 DEG C of heat treatment 180min, cooled to room temperature is to get to transparent glass-ceramics.
Under similarity condition, 120,100 and 0min is replaced in 423 DEG C of heat treatment times.
Infrared lumious material has good translucency, and nanocrystal in rear-earth-doped devitrified glass described in the present embodiment
It is evenly distributed in substrate glass (referring to Fig. 3 a), from rare earth ion known to the luminous map of Fig. 7 in the environment of nanocrystal field
Middle luminous intensity has been up to 8 times or more through Overheating Treatment 30min microcrystal glass material.
Embodiment 4
By composition 90TeO2-5Nb2O5-5Bi2O3(mol%) TeO needed for weighing 60g2,Nb2O5,Bi2O3,Er2O3Powder raw material
(purity 99.99%), Er2O3According to 0.2mol% is mixed outside molar ratio, it is fitted into after being sufficiently mixed in crucible with cover and is placed in 850 DEG C
60min is melted, is then quickly cast to glass solution on the Stainless Molding Board for having been preheated with 350 DEG C, in Muffle after molding
Two hours are kept the temperature for 380 DEG C in furnace, and temperature is cooled to by room temperature with the speed of 5 DEG C/min, obtains the tellurium bismuthates containing rare earth ion
Glass, and obtained glass cut, polishing treatment；The obtained tellurium bismuthate glass containing rare earth ion is existed
400 DEG C are nearby heat-treated 12h, and then in 426 DEG C of heat treatment 180min, cooled to room temperature is to get to transparent glass-ceramics.
Under similarity condition, 120,100 and 0min is replaced in 426 DEG C of heat treatment times.
Infrared lumious material has good translucency, and nanocrystal in rear-earth-doped devitrified glass described in the present embodiment
It is evenly distributed in substrate glass (referring to Fig. 3 a), from rare earth ion known to the luminous map of Fig. 8 in the environment of nanocrystal field
Middle luminous intensity has been up to 18 times or more through Overheating Treatment 30min microcrystal glass material.
The foregoing is only a preferred embodiment of the present invention, not does restriction in any form to the present invention.It is all
Any equivalent variation that those skilled in the art makes above-described embodiment using technical solution of the present invention is modified or is drilled
Become etc., all of which are still within the scope of the technical scheme of the invention.
Claims (8)
1. a kind of middle infrared lumious material of rear-earth-doped devitrified glass, which is characterized in that the base of the middle infrared lumious material
This raw material composition are as follows:
TeO265 ~ 90mol%,
Bi2O35 ~ 15mol%,
Nb2O55 ~ 20mol%,
Said components and be 100mol%；
The basic raw material is also outer to adulterate Er2O3, doping is the 0.2-0.75mol% of basic raw material composition.
2. the preparation method of infrared lumious material in rear-earth-doped devitrified glass described in claim 1, it is characterised in that including
Following steps:
(1) raw material is sufficiently mixed, stirring carries out melted, and the liquid of melting is poured into stainless steel punching block, Muffle is then placed in
It anneals after furnace heat preservation, then cools to room temperature, obtain the glass containing rare earth ion, and obtained glass is cut
And polishing treatment；
(2) glass containing rare earth ion after polishing treatment is heat-treated in Tg ± 2 DEG C, continues heating lower than crystallization temperature 2-
5 DEG C of heat treatments, then cooled to room temperature is to get the infrared lumious material into the rear-earth-doped devitrified glass.
3. preparation method according to claim 2, which is characterized in that in the step (1), glass melting temperature is 800 ~ 1000
DEG C, melting time is 30 ~ 60min.
4. preparation method according to claim 2, which is characterized in that in the step (1), stainless steel punching block is preheated to
200~350℃。
5. preparation method according to claim 2, which is characterized in that in the step (1), in Muffle furnace temperature be 370 ~
390 DEG C, keep the temperature 2h-4h.
6. preparation method according to claim 2, which is characterized in that in the step (1), cooling velocity be 5 ~ 10 DEG C/
min。
7. preparation method according to claim 2, which is characterized in that in the step (2), be heat-treated 8- in Tg ± 2 DEG C
12h。
8. preparation method according to claim 2, which is characterized in that in the step (2), be lower than crystallization temperature 3-5
DEG C heat treatment 90-180min.
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| CN110228948A (en) * | 2019-05-14 | 2019-09-13 | 重庆邮电大学 | A kind of novel photoluminescent transparent glass ceramics and preparation method thereof |
| CN110540362A (en) * | 2019-09-25 | 2019-12-06 | 华南理工大学 | Perovskite quantum dot doped glass with reversible luminescence and preparation method thereof |
| CN111606562A (en) * | 2020-05-27 | 2020-09-01 | 武汉理工大学 | Preparation method of intermediate infrared luminescent rare earth doped fluoride nanocrystalline glass material |
| CN111847886A (en) * | 2020-07-01 | 2020-10-30 | 暨南大学 | Tin dioxide-containing nano microcrystalline glass and preparation method thereof |
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